CN106220221A - A kind of supporter preparation method and applications for synthesizing molecular sieve film - Google Patents
A kind of supporter preparation method and applications for synthesizing molecular sieve film Download PDFInfo
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- CN106220221A CN106220221A CN201610617669.4A CN201610617669A CN106220221A CN 106220221 A CN106220221 A CN 106220221A CN 201610617669 A CN201610617669 A CN 201610617669A CN 106220221 A CN106220221 A CN 106220221A
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- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/20—Faujasite type, e.g. type X or Y
- C01B39/24—Type Y
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
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Abstract
The present invention relates to the preparation method of a kind of high intensity molecular sieve film support, using the mixture of alumina powder and sa powder as ceramic aggregate, the size utilizing the particle diameter between two kinds of powders is allocated, prepare that performance is controlled, particle packing and pore distribution uniformly and the supporter of beneficially molecular screen membrane growth.The inventive method technique simple economy, applied widely.
Description
Technical field
The present invention relates to the preparation method of a kind of porous ceramic support, particularly to the synthesis of a kind of applicable molecular screen membrane
The preparation method of supporter, and its application in being applied to molecular screen membrane preparation.
Background technology
Molecular screen membrane is the inorganic material film that a class has regular microchannel structure, such membrane material aperture at below 1nm,
The adsorptive selectivity in its duct and molecular sieving characteristics make it have a very wide range of applications at intermolecular separation field.Molecular sieve
The synthesis of film need to be on the basis of the porous supporting body that applicable molecular sieve crystal grows, therefore structure, the mechanicalness to supporter
Energy etc. has the highest requirement.In general can make to support by interpolation nano aluminium oxide, titanium oxide etc. in ceramic aggregate
The intensity of body improves, but this method would generally reduce porosity and the permeability of supporter.
The patent of publication number CN101913873A provides a kind of porous ceramics mistake that can improve intensity and pore connectivity
The preparation method of chimney filter supporter, by make aggregate with the reasonable layout of various additives thus improve supporter sinter after strong
Degree, but mainly improve the uniformity of intensity distributions.
Summary of the invention
It is an object of the invention to: provide one to prepare performance is controlled, particle packing and pore distribution more uniform
For the supporter preparation method of synthesizing molecular sieve film, mainly by the interaction of alumina powder Yu sa powder,
Can prepare, by the size of two kinds of powders and match ratio, the molecular screen membrane supporter that performance is controlled simultaneously.Particular content
Including following aspect:
A kind of supporter preparation method for synthesizing molecular sieve film, comprises the steps:
1), by alumina powder and sa powder mix homogeneously, as aggregate;
2), in aggregate, addition pore creating material, binding agent, plasticizer and lubricant stir, then prepare pug after old;
3), again by pug through vacuum pugging, extrusion molding, dry, sinter prepared porous molecular screen film support.
Described alumina powder is white fused alumina, α-Al2O3, the mixture of one or more in aluminium hydroxide;Described sial
Matter powder is the mixture of one or more in mullite, Kaolin, gangue, bauxite;Alumina powder and/or sial
The mean diameter of matter powder is 1~15 μm.
The weight ratio of alumina powder and sa powder is 1:(0.1~10), preferably 1:(0.2~6), preferably 1:
(0.4~4).
Described pore creating material is one or more the combination in activated carbon powder, starch or cellulose family, described pore-creating
Agent mean diameter is less than aggregate, and addition is the 1~15% of aggregate quality.
Described binding agent is one or more the combination in paraffin, dextrin or cellulose family;Plasticizer is poly-
Alcohols, lubricant is the oils such as glycerol, Oleum Verniciae fordii, soybean oil;The addition of binding agent, plasticizer or lubricant is respectively bone
The 0~15wt% of the weight of material, more preferably 0.5~10wt%, more preferably 1~10wt%.
Described sintering temperature is 1200~1600 DEG C, and the sintered heat insulating time is 1~12h.
The application in preparing molecular screen membrane of the described supporter, including the preparation of NaA type, T-shaped, y-type zeolite membrane etc..
Beneficial effect
Compound by alumina powder and sa powder, by both size and the regulation and control of match ratio, can prepare
Performance is controlled, the more uniform molecular screen membrane supporter of particle packing and pore distribution.The inventive method technique simple economy, removes
It is applicable to outside the preparation of molecular screen membrane, is also applied for the preparation of other ceramic filtration membrane, applied widely.Support prepared by the present invention
Body porosity of=38%, average pore size 0.2~5 μm, 3 rupture strength >=70MPa.
Accompanying drawing explanation
Fig. 1 is the electron micrograph of the supporter of embodiment 1 preparation.
Fig. 2 is the electron micrograph of the supporter of reference examples 1 preparation.
Fig. 3 a, b are respectively surface and the section ultramicroscope photograph of the molecular screen membrane of the supporter synthesis of embodiment 1 preparation
Sheet.
Detailed description of the invention
Embodiment 1
1) by α-Al that 5kg average pore size is 6 μm2O3Powder, 5kg average pore size are mullite fine powder and the 500g grain of 6 μm
Footpath is less than the activated carbon mix homogeneously of 6 μm;
2) while stirring in the mixed powder that step 1) obtains add 500g hydroxypropyl methyl cellulose, 1kg Polyethylene Glycol,
1kg glycerol, stirs, old 12 hours prepared pugs;
3) pug is prepared the single-tube wet base of porous molecular screen film support through vacuum pugging, extrusion molding;
4) being dried by wet base, burn till at 1480 DEG C, temperature retention time is 4 hours, then natural cooling, obtains molecular screen membrane and supports
Body.
The supporter obtained is through characterizing, and average pore size is 1.3 μm, porosity 40%, 3 rupture strength 85Mpa.
Embodiment 2
1) by 6kg mean diameter be the white alundum powder of 5 μm, 4kg mean diameter be that the Kaolin of 3 μm and 450g particle diameter are less than 3 μ
The starch mix homogeneously of m;
2) in the mixed powder that step 1) obtains, 500g paraffin, 1kg polyvinyl alcohol, 1kg Oleum Verniciae fordii, stirring are added while stirring
Uniformly, old 24 hours prepared pugs;
3) pug is prepared the four-way channel type wet base of porous molecular screen film support through vacuum pugging, extrusion molding;
4) being dried by wet base, burn till at 1550 DEG C, temperature retention time is 6 hours, then natural cooling, obtains molecular screen membrane and supports
Body.
The supporter obtained is through characterizing, and average pore size is 1.5 μm, porosity 38%, 3 rupture strength 98MPa.
Embodiment 3
1) alpha-aluminium oxide powder that 8kg mean diameter is 2 μm made, 2kg mean diameter is the gangue of 5 μm and 600g particle diameter is little
Activated carbon mix homogeneously in 2 μm;
2) in the mixed powder that step 1) obtains, nano-titanium oxide, the 500g stone that 400g content is 40% is added while stirring
Wax, 800g Polyethylene Glycol, 1.2kg glycerol, stir, old 24 hours prepared pugs;
3) pug is prepared the single hose wet base of porous molecular screen film support through vacuum pugging, extrusion molding;
4) being dried by wet base, burn till at 1200 DEG C, temperature retention time is 2 hours, then natural cooling, obtains molecular screen membrane and supports
Body.
Reference examples 1
Difference with embodiment 1 is: use α-Al in aggregate completely2O3Powder.
1) by α-Al that 10kg average pore size is 6 μm2O3Powder and 500g particle diameter are less than the activated carbon mix homogeneously of 6 μm;
2) while stirring in the mixed powder that step 1) obtains add 500g hydroxypropyl methyl cellulose, 1kg Polyethylene Glycol,
1kg glycerol, stirs, old 12 hours prepared pugs;
3) pug is prepared the single-tube wet base of porous molecular screen film support through vacuum pugging, extrusion molding;
4) being dried by wet base, burn till at 1480 DEG C, temperature retention time is 4 hours, then natural cooling, obtains molecular screen membrane and supports
Body.
The supporter obtained is through characterizing, and average pore size is 1.1 μm, porosity 28%, 3 rupture strength 61Mpa.
Reference examples 2
Difference with embodiment 1 is: use mullite fine powder in aggregate completely.
1) mullite fine powder and 500g particle diameter that 10kg average pore size is 6 μm are mixed all less than the activated carbon of 6 μm
Even;
2) while stirring in the mixed powder that step 1) obtains add 500g hydroxypropyl methyl cellulose, 1kg Polyethylene Glycol,
1kg glycerol, stirs, old 12 hours prepared pugs;
3) pug is prepared the single-tube wet base of porous molecular screen film support through vacuum pugging, extrusion molding;
4) being dried by wet base, burn till at 1480 DEG C, temperature retention time is 4 hours, then natural cooling, obtains molecular screen membrane and supports
Body.
The supporter obtained is through characterizing, and average pore size is 1.5 microns, porosity 28%, 3 rupture strength 56MPa.
Table 1 embodiment and reference examples supporter performance comparison
The supporter porosity relatively reference examples that as can be seen from Table 1 prepared by embodiment improves more than 35%, and intensity improves more than 39%.
Supporter application test:
Above-mentioned supporter is applied to the preparation of NaA molecular sieve membrane, membrane preparation method reference: the system of a kind of NaA molecular sieve membrane
Preparation Method and device (CN105056769A).Carried out by the NaA molecular sieve membrane of supporter gained in embodiment and reference examples respectively
Infiltration evaporation is implemented, and experimental condition is: operation temperature 70 DEG C, separation system is the ethanol/water solution of 5 wt.%.Acquired results
As shown in table 2.
The infiltration evaporation experimental result of the molecular screen membrane synthesized by each embodiment of table 2
As can be seen from the table, above-mentioned supporter is used can to synthesize the perfect sunken NaA molecular sieve membrane in surface, its point
From the factor > 5000, flux > 2.5kg h–1·m–2, with high selectivity and permeation flux, it is better than reference examples sample.
Claims (10)
1. the supporter preparation method for synthesizing molecular sieve film, it is characterised in that comprise the steps: 1), will oxidation
Aluminium powder material and sa powder mix homogeneously, as aggregate;2), in aggregate, pore creating material, binding agent, plasticizer and lubrication are added
Agent stirs, then prepares pug after old;3), again by pug through vacuum pugging, extrusion molding, dry, sinter prepare many
Porous molecular sieve film support.
Supporter preparation method for synthesizing molecular sieve film the most according to claim 1, it is characterised in that described oxidation
Aluminium powder material is white fused alumina, α-Al2O3, the mixture of one or more in aluminium hydroxide;Described sa powder be mullite,
The mixture of one or more in Kaolin, gangue, bauxite;Alumina powder and/or the average particle of sa powder
Footpath is 1~15 μm.
Supporter preparation method for synthesizing molecular sieve film the most according to claim 1, it is characterised in that alumina powder
The weight ratio of material and sa powder is 1:0.1~10, more preferably 1:0.2~6.
Supporter preparation method for synthesizing molecular sieve film the most according to claim 1, it is characterised in that described pore-creating
Agent is one or more the combination in activated carbon powder, starch or cellulose family, and described pore creating material mean diameter is less than bone
Material, addition is the 1~15% of aggregate quality.
Supporter preparation method for synthesizing molecular sieve film the most according to claim 1, it is characterised in that described bonding
Agent is one or more the combination in paraffin, dextrin or cellulose family;Plasticizer is polyalcohols, and lubricant is sweet
The oils such as oil, Oleum Verniciae fordii, soybean oil;The addition of binding agent, plasticizer or lubricant be respectively the weight of aggregate 0~
15wt%, more preferably 0.5~10wt%.
Supporter preparation method for synthesizing molecular sieve film the most according to claim 1, it is characterised in that described sintering
Temperature is 1200~1600 DEG C, and the sintered heat insulating time is 1~12h.
Supporter preparation method for synthesizing molecular sieve film the most according to claim 1, it is characterised in that prepared
Supporter is tubular type, flat, hollow fiber form etc..
8. the supporter that the supporter preparation method for synthesizing molecular sieve film described in any one of claim 1~7 obtains.
9. the application in preparing molecular screen membrane of the supporter described in claim 8.
Application the most according to claim 9, it is characterised in that the film layer of molecular screen membrane is selected from NaA type, T-shaped, Y type molecule
Sieve membrane etc..
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108484149A (en) * | 2018-03-30 | 2018-09-04 | 滁州学院 | A kind of NaA molecular sieve film support preparation method |
CN109433020A (en) * | 2018-12-27 | 2019-03-08 | 延海港 | It is a kind of for the industrial solvent dehydration preparation method of tubular type membrane material |
CN111646785A (en) * | 2020-06-15 | 2020-09-11 | 吉林大学 | Porous alumina film, silver ion-containing porous alumina composite film and preparation method thereof |
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JP5068788B2 (en) * | 2009-07-10 | 2012-11-07 | 三井造船株式会社 | One-end-sealed zeolite membrane substrate tube |
CN104987120A (en) * | 2015-07-21 | 2015-10-21 | 江苏九天高科技股份有限公司 | Molecular sieve membrane support body preparation method |
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2016
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Publication number | Priority date | Publication date | Assignee | Title |
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JP5068788B2 (en) * | 2009-07-10 | 2012-11-07 | 三井造船株式会社 | One-end-sealed zeolite membrane substrate tube |
CN104987120A (en) * | 2015-07-21 | 2015-10-21 | 江苏九天高科技股份有限公司 | Molecular sieve membrane support body preparation method |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108484149A (en) * | 2018-03-30 | 2018-09-04 | 滁州学院 | A kind of NaA molecular sieve film support preparation method |
CN108484149B (en) * | 2018-03-30 | 2020-12-01 | 滁州学院 | Preparation method of NaA molecular sieve membrane support |
CN109433020A (en) * | 2018-12-27 | 2019-03-08 | 延海港 | It is a kind of for the industrial solvent dehydration preparation method of tubular type membrane material |
CN111646785A (en) * | 2020-06-15 | 2020-09-11 | 吉林大学 | Porous alumina film, silver ion-containing porous alumina composite film and preparation method thereof |
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